Sodium Carbonate → Methyl 6-[(2,2-diphenylethyl)amino]-9-{(2R,3R,4S,5S)-5-[(ethylamino)carbonyl]-3,4-dihydroxytetrahydro-2-furanyl}-9H-purine-2-carboxylate

HRID 1060552

反応式

HRID 1060552 の反応式
C([O:9][C@@H:10]1[C@@H:14]([O:15]C(=O)C2C=CC=CC=2)[C@@H:13]([C:24]([NH:26][CH2:27][CH3:28])=[O:25])[O:12][C@H:11]1[N:29]1[CH:37]=[N:36][C:35]2[C:30]1=[N:31][C:32]([C:53]([O:55][CH3:56])=[O:54])=[N:33][C:34]=2[NH:38][CH2:39][CH:40]([C:47]1[CH:52]=[CH:51][CH:50]=[CH:49][CH:48]=1)[C:41]1[CH:46]=[CH:45][CH:44]=[CH:43][CH:42]=1)(=O)C1C=CC=CC=1.C(=O)([O-])[O-].[Na+].[Na+]>CO>[C:47]1([CH:40]([C:41]2[CH:42]=[CH:43][CH:44]=[CH:45][CH:46]=2)[CH2:39][NH:38][C:34]2[N:33]=[C:32]([C:53]([O:55][CH3:56])=[O:54])[N:31]=[C:30]3[C:35]=2[N:36]=[CH:37][N:29]3[C@H:11]2[C@H:10]([OH:9])[C@H:14]([OH:15])[C@@H:13]([C:24]([NH:26][CH2:27][CH3:28])=[O:25])[O:12]2)[CH:48]=[CH:49][CH:50]=[CH:51][CH:52]=1

参加物

4

反応物 2

HCID 10340Sodium CarbonateHCID 18345898methyl 9-{(2R,3R,4R,5S)-3,4-bis(benzoyloxy)-5-[(ethylamino)carbonyl]-tetrahydro-2-furanyl}-6-[(2,2-diphenylethyl)amino]-9H-purine-2-carboxylate

生成物 1

HCID 10187396Methyl 6-[(2,2-diphenylethyl)amino]-9-{(2R,3R,4S,5S)-5-[(ethylamino)carbonyl]-3,4-dihydroxytetrahydro-2-furanyl}-9H-purine-2-carboxylate収率 97.6%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

A solution of methyl 9-{(2R,3R,4R,5S)-3,4-bis(benzoyloxy)-5-[(ethylamino)carbonyl]-tetrahydro-2-furanyl}-6-[(2,2-diphenylethyl)amino]-9H-purine-2-carboxylate (Preparation 10) (3.4 g, 4.5 mmol) and sodium carbonate (50 mg) in dry methanol (60 ml) was stirred at room temperature for four hours. The solvent was removed under reduced pressure and the residue was taken up in a mixture of dichloromethane:methanol (95:5 by volume, 60 ml). Inorganic salts were filtered off and the filtrate was evaporated under reduced pressure. The residue was triturated with ether, filtered off and dried to yield the target compound as a white solid (2.4 g).

後処理

  1. customThe solvent was removed under reduced pressure
  2. additionthe residue was taken up in a mixture of dichloromethane:methanol (95:5 by volume, 60 ml)
  3. filtrationInorganic salts were filtered off
  4. customthe filtrate was evaporated under reduced pressure
  5. customThe residue was triturated with ether
  6. filtrationfiltered off
  7. customdried

出典と根拠

ORDレコード
ord-db61013a99524ec0ae08eedc141c61cf
出典データセット
uspto-grants-2003_02
特許番号
US06525032B2

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